A new methane partial oxidation (MPO) catalyst has been prepared by grafting MoO2(acac)(2) (acac: acetylacetonate ligand) onto the surface of dried HZSM-5 zeolite. This reaction was performed in an organic solvent under an inert atmosphere with the exclusion of water from the reaction. It was shown by FT-IR spectroscopy that the reaction takes place between the acidic hydroxyl groups of the zeolite and the acetylacetonate ligands of the complex. After the grafting reaction, the solid was washed, dried and calcined in air, to afford the final [S]O2MoO2, Mo(VI), highly dispersed, surface species. The catalytic activity of this new material in the MPO reaction is enhanced in comparison with the classical Mo,W/HZSM-5 impregnation catalysts.